十二烷基甲基二甲氧基硅烷偶联剂的合成研究

Study on Synthesis of Dodecylmethyldimethoxysilane Silane Coupling Agent

摘要:

以甲基二氯硅烷和1-十二烯为原料，在自制铂催化剂作用下合成中间体十二烷基甲基二氯硅烷，再经无溶剂气-液相反应法醇解得到十二烷基甲基二甲氧基硅烷，对目的产物行了1HNMR、IR 表征。经单因素实验分别确定了硅氢加成和醇解反应的最佳条件：在1-十二烯进料速度5mL/min、n(甲基二氯硅烷)∶n(1-十二烯)=1.1∶1、m(铂催化剂)∶m(甲基二氯硅烷)=1.5×10﹣4∶1、反应温度110℃条件下反应20min，十二烷基甲基二氯硅烷的收率可达92.5%，β-加成产物的选择性为100%；在中间体进料速度1mL/min、甲醇蒸气流量1500 mL/min、反应温度85℃条件下，目的产物十二烷基甲基二甲氧基硅烷经分离提纯后的质量分数为97%，收率可达90.5%。

Abstract:

Using methyldichlorosilane with 1-dodecene as materials have successfully synthesized dodecylmethyldimethoxysilane using self-made platinum catalyst, and then dodecylmethyldimethoxysilane was synthesised via alcoholysis reaction through atmospheric liquid-phase reaction. The structure of target compound was characterized by means of 1HNMR and IR spectrum. The reaction conditions have been optimized as follows: feeding speed of dodecene 5mL/min, n(methyldichlorosilane)∶n(1-dodecene)=1.1∶1, m(platinum catalyst)∶m(methyldichlorosilane) = 1.5×10﹣4∶1, reaction temperature 110℃, reaction time 20min and the yield of intermediate product could reached 92.5%, selectivity to β-addition product was 100%. Feeding speed of intermediate product 1mL/min, methanol steam flow 1500mL/min, eaction temperature 85℃, the purity of the dodecylmethyldimethoxysilane was 97% after the separation and purification processes，the yield of product could reached 90.5% .